CN102219242A - Method for preparing mesoporous aluminum oxide - Google Patents
Method for preparing mesoporous aluminum oxide Download PDFInfo
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- CN102219242A CN102219242A CN2010101468684A CN201010146868A CN102219242A CN 102219242 A CN102219242 A CN 102219242A CN 2010101468684 A CN2010101468684 A CN 2010101468684A CN 201010146868 A CN201010146868 A CN 201010146868A CN 102219242 A CN102219242 A CN 102219242A
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Abstract
The invention relates to a method for preparing mesoporous aluminum oxide, which mainly solves the problems that the preparation cost of the mesoporous aluminum oxide is high and the preparation operation is complicated in the prior art. The method adopts the following technical scheme for solving the problems: inorganic aluminum salt is taken as a raw material, P123 is taken as a template agent, inorganic ammonia or inorganic ammonium salt is taken as a precipitating agent, the reaction is conducted under the condition that the pH value is 1-14 and the reacting temperature is 1-100 DEG C so as to obtain the mesoporous aluminum oxide, wherein the mole ratio of the inorganic aluminum salt to the P124 is 1-200:1, and the precipitating agent using amount is calculated according to the mole ratio of the inorganic aluminum salt, and is 1-50:1 of the mole ratio of the inorganic aluminum salt. The method can be used for industrial preparation of the mesoporous aluminum oxide.
Description
Technical field
The present invention relates to a kind of method for preparing meso-porous alumina.
Background technology
Activated alumina is a kind of porousness solid material, has that specific surface area and pore volume are big, pore distribution is adjustable, a physical strength height after the moulding, and advantages such as Heat stability is good and source are abundant, price cheapness are widely used as support of the catalyst in catalytic field.Its structural parameter such as specific surface area, pore volume, pore size distribution etc. are closely related with selectivity of catalyst, activity and life-span, and the improvement of these physical parameters can improve the active ingredient dispersity, effectively promote mass transfer process in the reaction.And the meso-porous alumina pore size distribution is narrower, and specific surface area is bigger, and the different electromotive force in surface makes the easier load of different metal ions.Simultaneously, meso-porous alumina also has fabulous application potential as shape-selective catalyst, molecular sieve and selective adsorption or biochemical technology field aspect molecular recognition.
Synthesizing of mesoporous aluminum oxide material, template, activated aluminum powder hydrolysis method, exsiccated ammonium alum method, sol-gel method etc. are arranged at present, it is more wherein with the tensio-active agent to be that template prepares alumina material research, tensio-active agent wherein mainly contains ionic surface active agent (as Sodium dodecylbenzene sulfonate, cetyl trimethylammonium bromide) and nonionogenic tenside (as P123-tensio-active agent, full name is a polyoxyethylene-poly-oxypropylene polyoxyethylene, molecular formula is: PEO-PPO-PEO, molecular-weight average are 3500～8000) etc.When making template borolon material with organism such as tensio-active agents, at present in the bibliographical information aluminium source many be raw material with the alkoxide, prepare the alumina material that has than bigger serface and different apertures, but its raw material costliness, reaction is complicated.There have bibliographical information with the inorganic aluminate to be that raw material and sucrose carry out to be molten altogether, and high-temperature roasting obtains in the method for alumina again, and all there is the deficiency of self in the mol ratio of sucrose and aluminium salt up to 250 times.
Find that through literature search a large amount of synthetic Al is arranged at present to prior art
2O
3The bibliographical information of material.Zhang Bo is at " Dalian Railway University's journal " 2006,27 (1), " preparation of P123 template aluminum oxide mesoporous material and the performance " delivered on the 71-75, mention with the aluminum isopropylate being the aluminium source in this article, drip an amount of nitric acid earlier and form colloidal sol, stirring in water bath takes by weighing P123 it is dissolved in the above-mentioned colloidal sol then, continue to stir to move in the autoclave after 1 hour and carried out hydro-thermal reaction 24 hours, obtain meso-porous alumina.Adopting organic aluminium salt in the document is the aluminium source, has the preparation cost height, in addition the problem of complicated operation.
Summary of the invention
Technical problem to be solved by this invention is the problem that has preparation cost height, complicated operation in the prior art, and a kind of new mesoporous alumina preparation method is provided.This method has low, the simple to operate advantage of preparation cost.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of method for preparing meso-porous alumina, with the inorganic aluminate is raw material, with P123 is template, with inorganic ammonia or inorganic ammonium salt is precipitation agent, be made into mixing solutions, in the pH value is 1～14, temperature of reaction is to react under 1～100 ℃ of condition, reaction product obtains meso-porous alumina through filtration, drying and 300～700 ℃ of roastings, wherein the mol ratio of inorganic aluminate and P123 is 1～200: 1, and the precipitation agent consumption is 1～50: 1 of an inorganic aluminate mol ratio with the inorganic aluminate molar ratio computing.
In the technique scheme, the inorganic aluminate preferred version is selected from least a in aluminum nitrate, aluminum chloride or the Tai-Ace S 150, the mol ratio preferable range of inorganic aluminate and P123 is 25～100: 1, precipitation agent and inorganic aluminate, with inorganic aluminate molar ratio computing preferable range is 5～20: 1, the pH value of solution preferable range is 5～12 in the reaction, and the temperature of reaction preferable range is 20～50 ℃; Precipitation agent is selected from ammonia soln, volatile salt or ammonium bicarbonate soln.
The present invention is a raw material owing to adopt inorganic aluminate cheap, that be easy to get in preparation meso-porous alumina process, greatly reduces preparation cost, owing to adopt precipitator method prepared meso-porous alumina, makes the reaction times short, simple to operate in addition.The meso-porous alumina specific surface area that adopts method of the present invention to prepare is 180～400 meters
2/ gram, pore volume is 0.15～0.5 centimetre
3/ gram, pore size distribution is 3.5～7.6 nanometers, has obtained better technical effect.
The present invention is further elaborated below by embodiment.
Embodiment
[embodiment 1]
Pressed inorganic aluminate and P123 mol ratio 25: 1, wherein the molecular-weight average of P123 is 5800, takes by weighing 7.5026 grams, nine water aluminum nitrates, with the beaker of packing into of the raw material after the weighing, adds 50 ml deionized water, and 20 ℃ are stirred down and dissolved in 30 minutes; Slowly splash into 48 milliliters of P123 solution then, above-mentioned solution mixed after 30 minutes, dripped 2.5% ammonia soln again, and regulator solution pH=9 continues to stir after 1 hour washing, suction filtration.
After draining, take out sample and put into air dry oven, under 100 ℃ of conditions of oven temperature, be incubated 6 hours, sample is taken out in dry back.Sample after the drying is inserted in the retort furnace of band temperature control, 500 ℃ of roastings 4 hours, the alumina material that obtains preparing is taken out in cooling.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 242 meters
2/ gram, pore volume is 0.32 centimetre
3/ gram, mean pore size is 6.8 nanometers.
[embodiment 2]
Pressed inorganic aluminate and P123 mol ratio 50: 1, wherein the molecular-weight average of P123 is 5800, takes by weighing 7.5026 grams, nine water aluminum nitrates, with the beaker of packing into of the raw material after the weighing, adds 50 ml deionized water, and 20 ℃ are stirred down and dissolved in 30 minutes; Slowly splash into 24 milliliters of P123 solution then, above-mentioned solution mixed after 30 minutes, dripped 2.5% ammonia soln again, and regulator solution pH=9 continues to stir after 1 hour washing, suction filtration.
After draining, take out sample and put into air dry oven, under 100 ℃ of conditions of oven temperature, be incubated 6 hours, sample is taken out in dry back.Sample after the drying is inserted in the retort furnace of band temperature control, 500 ℃ of roastings 4 hours, the alumina material that obtains preparing is taken out in cooling.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 266 meters
2/ gram, pore volume is 0.39 centimetre
3/ gram, mean pore size is 5.9 nanometers.
[embodiment 3]
Pressed inorganic aluminate and P123 mol ratio 100: 1, wherein the molecular-weight average of P123 is 5800, takes by weighing 7.5026 grams, nine water aluminum nitrates, with the beaker of packing into of the raw material after the weighing, adds 50 ml deionized water, and 20 ℃ are stirred down and dissolved in 30 minutes; Slowly splash into 12 milliliters of P123 solution then, above-mentioned solution mixed after 30 minutes, dripped 2.5% ammonia soln again, and regulator solution pH=9 continues to stir after 1 hour washing, suction filtration.
After draining, take out sample and put into air dry oven, under 100 ℃ of conditions of oven temperature, be incubated 6 hours, sample is taken out in dry back.Sample after the drying is inserted in the retort furnace of band temperature control, 500 ℃ of roastings 4 hours, the alumina material that obtains preparing is taken out in cooling.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 284 meters
2/ gram, pore volume is 0.44 centimetre
3/ gram, mean pore size is 4.8 nanometers.
[embodiment 4]
Pressed inorganic aluminate and P123 mol ratio 50: 1, wherein the molecular-weight average of P123 is 3500, takes by weighing 7.5026 grams, nine water aluminum nitrates, with the beaker of packing into of the raw material after the weighing, adds 50 ml deionized water, and 20 ℃ are stirred down and dissolved in 30 minutes; Slowly splash into 24 milliliters of P123 solution then, above-mentioned solution mixed after 30 minutes, dripped 2.5% ammonia soln again, and regulator solution pH=5 continues to stir after 1 hour washing, suction filtration.
After draining, take out sample and put into air dry oven, under 100 ℃ of conditions of oven temperature, be incubated 6 hours, sample is taken out in dry back.Sample after the drying is inserted in the retort furnace of band temperature control, 500 ℃ of roastings 4 hours, the alumina material that obtains preparing is taken out in cooling.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 189 meters
2/ gram, pore volume is 0.31 centimetre
3/ gram, mean pore size is 3.9 nanometers.
[embodiment 5]
Pressed inorganic aluminate and P123 mol ratio 50: 1, wherein the molecular-weight average of P123 is 8000, takes by weighing 7.5026 grams, nine water aluminum nitrates, with the beaker of packing into of the raw material after the weighing, adds 50 ml deionized water, and 20 ℃ are stirred down and dissolved in 30 minutes; Slowly splash into 24 milliliters of P123 solution then, above-mentioned solution mixed after 30 minutes, dripped 2.5% ammonia soln again, and regulator solution pH=12 continues to stir after 1 hour washing, suction filtration.
After draining, take out sample and put into air dry oven, under 100 ℃ of conditions of oven temperature, be incubated 6 hours, sample is taken out in dry back.Sample after the drying is inserted in the retort furnace of band temperature control, 500 ℃ of roastings 4 hours, the alumina material that obtains preparing is taken out in cooling.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 271 meters
2/ gram, pore volume is 0.44 centimetre
3/ gram, mean pore size is 6.5 nanometers.
[embodiment 6]
Pressed inorganic aluminate and P123 mol ratio 50: 1, wherein the molecular-weight average of P123 is 5800, takes by weighing 7.5026 grams, nine water aluminum nitrates, with the beaker of packing into of the raw material after the weighing, adds 50 ml deionized water, and 20 ℃ are stirred down and dissolved in 30 minutes; Slowly splash into 24 milliliters of P123 solution then, above-mentioned solution mixed after 30 minutes, dripped 2.5% ammonia soln again, and regulator solution pH=9 continues to stir after 1 hour washing, suction filtration.
After draining, take out sample and put into air dry oven, under 100 ℃ of conditions of oven temperature, be incubated 6 hours, sample is taken out in dry back.Sample after the drying is inserted in the retort furnace of band temperature control, 300 ℃ of roastings 4 hours, the alumina material that obtains preparing is taken out in cooling.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 251 meters
2/ gram, pore volume is 0.32 centimetre
3/ gram, mean pore size is 4.5 nanometers.
[embodiment 7]
Pressed inorganic aluminate and P123 mol ratio 50: 1, wherein the molecular-weight average of P123 is 5800, takes by weighing 7.5026 grams, nine water aluminum nitrates, with the beaker of packing into of the raw material after the weighing, adds 50 ml deionized water, and 20 ℃ are stirred down and dissolved in 30 minutes; Slowly splash into 24 milliliters of P123 solution then, above-mentioned solution mixed after 30 minutes, dripped 2.5% ammonia soln again, and regulator solution pH=9 continues to stir after 1 hour washing, suction filtration.
After draining, take out sample and put into air dry oven, under 100 ℃ of conditions of oven temperature, be incubated 6 hours, sample is taken out in dry back.Sample after the drying is inserted in the retort furnace of band temperature control, 700 ℃ of roastings 4 hours, the alumina material that obtains preparing is taken out in cooling.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 187 meters
2/ gram, pore volume is 0.36 centimetre
3/ gram, mean pore size is 7.6 nanometers.
[embodiment 8]
Pressed inorganic aluminate and P123 mol ratio 50: 1, wherein the molecular-weight average of P123 is 4800, takes by weighing 7.5026 grams, nine water aluminum nitrates, with the beaker of packing into of the raw material after the weighing, adds 50 ml deionized water, and 50 ℃ are stirred down and dissolved in 30 minutes; Slowly splash into 24 milliliters of P123 solution then, above-mentioned solution mixed after 30 minutes, dripped 2.5% ammonia soln again, and regulator solution pH=9 continues to stir after 1 hour washing, suction filtration.
After draining, take out sample and put into air dry oven, under 100 ℃ of conditions of oven temperature, be incubated 6 hours, sample is taken out in dry back.Sample after the drying is inserted in the retort furnace of band temperature control, 500 ℃ of roastings 4 hours, the alumina material that obtains preparing is taken out in cooling.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 263 meters
2/ gram, pore volume is 0.38 centimetre
3/ gram, mean pore size is 5.7 nanometers.
[embodiment 9]
Pressed inorganic aluminate and P123 mol ratio 50: 1, wherein the molecular-weight average of P123 is 5800, takes by weighing 7.5026 grams, nine water aluminum nitrates, with the beaker of packing into of the raw material after the weighing, adds 50 ml deionized water, and 20 ℃ are stirred down and dissolved in 30 minutes; Slowly splash into 24 milliliters of P123 solution then, above-mentioned solution mixed after 30 minutes, dripped 2.5% ammonium bicarbonate soln again, and regulator solution pH=9 continues to stir after 1 hour washing, suction filtration.
After draining, take out sample and put into air dry oven, under 100 ℃ of conditions of oven temperature, be incubated 6 hours, sample is taken out in dry back.Sample after the drying is inserted in the retort furnace of band temperature control, 500 ℃ of roastings 4 hours, the alumina material that obtains preparing is taken out in cooling.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 252 meters
2/ gram, pore volume is 0.46 centimetre
3/ gram, mean pore size is 6.3 nanometers.
[embodiment 10]
Pressed inorganic aluminate and P123 mol ratio 50: 1, wherein the molecular-weight average of P123 is 6500, takes by weighing 5.22 gram aluminum chloride, with the beaker of packing into of the raw material after the weighing, adds 50 ml deionized water, and 20 ℃ are stirred down and dissolved in 30 minutes; Slowly splash into 24 milliliters of P123 solution then, above-mentioned solution mixed after 30 minutes, dripped 2.5% ammonia soln again, and regulator solution pH=9 continues to stir after 1 hour washing, suction filtration.
After draining, take out sample and put into air dry oven, under 100 ℃ of conditions of oven temperature, be incubated 6 hours, sample is taken out in dry back.Sample after the drying is inserted in the retort furnace of band temperature control, 500 ℃ of roastings 4 hours, the alumina material that obtains preparing is taken out in cooling.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 277 meters
2/ gram, pore volume is 0.43 centimetre
3/ gram, mean pore size is 6.9 nanometers.
[embodiment 11]
Pressed inorganic aluminate and P123 mol ratio 50: 1, wherein the molecular-weight average of P123 is 5800, takes by weighing 6.0 gram Tai-Ace S 150, with the beaker of packing into of the raw material after the weighing, adds 50 ml deionized water, and 20 ℃ are stirred down and dissolved in 30 minutes; Slowly splash into 24 milliliters of P123 solution then, above-mentioned solution mixed after 30 minutes, dripped 2.5% ammonia soln again, and regulator solution pH=9 continues to stir after 1 hour washing, suction filtration.
After draining, take out sample and put into air dry oven, under 100 ℃ of conditions of oven temperature, be incubated 6 hours, sample is taken out in dry back.Sample after the drying is inserted in the retort furnace of band temperature control, 500 ℃ of roastings 4 hours, the alumina material that obtains preparing is taken out in cooling.Pass through N
2Adsorption experiment and pore size distribution curve as can be known, the specific surface area of gained alumina material is 256 meters
2/ gram, pore volume is 0.39 centimetre
3/ gram, mean pore size is 5.7 nanometers.
Claims (7)
1. method for preparing meso-porous alumina, with the inorganic aluminate is raw material, with P123 is template, with inorganic ammonia or inorganic ammonium salt is precipitation agent, is made into mixing solutions, is 1～14 in the pH value, temperature of reaction is to react under 1～100 ℃ of condition, reaction product obtains meso-porous alumina through filtration, drying and 300～700 ℃ of roastings, and wherein the mol ratio of inorganic aluminate and P123 is 1～200: 1, and the precipitation agent consumption is 1～50: 1 of an inorganic aluminate mol ratio with the inorganic aluminate molar ratio computing.
2. the preparation method of meso-porous alumina according to claim 1 is characterized in that inorganic aluminate is selected from least a in aluminum nitrate, aluminum chloride or the Tai-Ace S 150, and the mol ratio of inorganic aluminate and P123 is 25～100: 1; The molecular-weight average of P123 is 3500～8000.
3. the preparation method of meso-porous alumina according to claim 1 is characterized in that the consumption of precipitation agent is 5～20: 1 of an inorganic aluminate mol ratio with the inorganic aluminate molar ratio computing.
4. the preparation method of meso-porous alumina according to claim 1 is characterized in that the pH value of solution value is 5～12.
5. the preparation method of meso-porous alumina according to claim 1 is characterized in that temperature of reaction is 20～50 ℃.
6. the preparation method of meso-porous alumina according to claim 1 is characterized in that precipitation agent is selected from ammonia soln, volatile salt or bicarbonate of ammonia.
7. the preparation method of the described meso-porous alumina of claim 1, the specific surface area that it is characterized in that meso-porous alumina is 180～400 meters
2/ gram, pore volume is 0.15～0.5 centimetre
3/ gram, pore size distribution is 3.5～7.6 nanometers.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701247A (en) * | 2012-05-08 | 2012-10-03 | 山东大学 | Preparation method of mesoporous spherical aluminum oxide |
| CN103896318A (en) * | 2014-04-02 | 2014-07-02 | 中国石油大学(华东) | Preparation method of bronsted acid-rich mesoporous alumina |
| CN106186014A (en) * | 2016-07-21 | 2016-12-07 | 中国石油大学(华东) | A kind of mesoporous γ Al2O3 synthetic method of function admirable |
| CN106219582A (en) * | 2016-07-21 | 2016-12-14 | 中国石油大学(华东) | A kind of preparation method with super large mesoporous pore volume γ Al2O3 |
| CN106669646A (en) * | 2016-11-28 | 2017-05-17 | 中国石油天然气股份有限公司 | B acid-enriched mesoporous alumina, as well as preparation method and application thereof |
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| CN101492170A (en) * | 2009-02-26 | 2009-07-29 | 同济大学 | Method of manufacturing mesoporous nano- aluminum oxide |
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| WO2009068117A1 (en) * | 2007-11-30 | 2009-06-04 | Nanologica Ab | Method for manufacturing a nanoporous alumina based materials with controlled textural and particle size and nanoporous alumina obtained by said method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102701247A (en) * | 2012-05-08 | 2012-10-03 | 山东大学 | Preparation method of mesoporous spherical aluminum oxide |
| CN103896318A (en) * | 2014-04-02 | 2014-07-02 | 中国石油大学(华东) | Preparation method of bronsted acid-rich mesoporous alumina |
| CN106186014A (en) * | 2016-07-21 | 2016-12-07 | 中国石油大学(华东) | A kind of mesoporous γ Al2O3 synthetic method of function admirable |
| CN106219582A (en) * | 2016-07-21 | 2016-12-14 | 中国石油大学(华东) | A kind of preparation method with super large mesoporous pore volume γ Al2O3 |
| CN106186014B (en) * | 2016-07-21 | 2019-07-09 | 中国石油大学(华东) | A kind of mesoporous γ-Al2O3 synthetic method of function admirable |
| CN106219582B (en) * | 2016-07-21 | 2019-07-09 | 中国石油大学(华东) | A kind of preparation method for holding γ-Al2O3 with super large mesoporous hole |
| CN106669646A (en) * | 2016-11-28 | 2017-05-17 | 中国石油天然气股份有限公司 | B acid-enriched mesoporous alumina, as well as preparation method and application thereof |
| CN106669646B (en) * | 2016-11-28 | 2019-06-11 | 中国石油天然气股份有限公司 | A kind of meso-porous alumina and its preparation method and application rich in B acid |
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